X-ray Diffraction Measurements Research Articles

Zn2-xGeO4-GeO2:(x)Mn2+ films with long persistence, intense brightness and high quantum efficiency, deposited by ultrasonic spray pyrolysis

This work shows the synthesis and characterization of the Zn2-xGeO4-GeO2:(x)Mn2+ (x = 0.10, 0.25, and 0.50 at.%) films using the Ultrasonic Spray Pyrolysis (USP) technique. These films were deposited at 500 °C and heat treated at 800 °C for 13 h. X-ray diffraction (XRD) measurements showed the rhombohedral and hexagonal phases of Zn2-xGeO4 (78.8 %) and GeO2 (21.2 %), respectively. SEM micrographs exhibited the surface morphology of these films. The STEM and HAADF show Ge, Zn, and O atomic layers. In addition, XPS was carried out to observe the oxidation states of Mn2+ (75.4 %) and Mn3+ (24.6 %) for the films doped with Mn ions (0.10 at.%). Incorporating manganese ions into the Zn2-xGeO4-GeO2 host lattice generated an extremely green emission, exciting at 250 nm. The photoluminescence and persistence luminescence properties were studied in accordance with the manganese doping concentration. For photoluminescence, it was found that the optimal doping percentage was 0.25 at.%, and for persistence luminescence, it was 0.10 at.% Mn with λex = 250 nm. Quantum efficiency measurements gave a result of 100 %. In addition, preliminary CL measurements were exhibited.

Developing time-resolved x-ray diffraction diagnostics at the National Ignition Facility (invited).

As part of a program to measure phase transition timescales in materials under dynamic compression, we have designed new x-ray imaging diagnostics to record multiple x-ray diffraction measurements during a single laser-driven experiment. Our design places several ns-gated hybrid CMOS (hCMOS) sensors within a few cm of a laser-driven target. The sensors must be protected from an extremely harsh environment, including debris, electromagnetic pulses, and unconverted laser light. Another key challenge is reducing the x-ray background relative to the faint diffraction signal. Building on the success of our predecessor (Target Diffraction In Situ), we implemented a staged approach to platform development. First, we built a demonstration diagnostic (Gated Diffraction Development Diagnostic) with two hCMOS sensors to confirm we could adequately protect them from the harsh environment and also acquire acceptable diffraction data. This allowed the team to quickly assess the risks and address the most significant challenges. We also collected scientifically useful data during development. Leveraging what we learned, we recently developed a much more ambitious instrument (Flexible Imaging Diffraction Diagnostic for Laser Experiments) that can field up to eight hCMOS sensors in a flexible geometry and participate in back-to-back shots at the National Ignition Facility (NIF). The design also allows for future iterations, such as faster hCMOS sensors and an embedded x-ray streak camera. The enhanced capabilities of the new instrument required a much more complex design, and the unexpected issues encountered on the first few shots at NIF remind us that complexity has consequences. Our progress in addressing these challenges is described herein, as is our current focus on improving data quality by reducing x-ray background and quantifying the uncertainties of our diffraction measurements.

Copper oxide–ferric oxide nanocomposite: Synthesis, characterization, and antibacterial and antifungal properties

Abstract Recently, copper oxide–ferric oxide nanocomposites (CuO/Fe2O3-NCs) have gained popularity and are widely employed in various applications. However, their effectiveness against phytopathogens has not been studied yet. This study investigates the synthesis and characterization of CuO/Fe2O3-NCs using the hydrothermal technique. X-ray diffraction (XRD), transmission electron microscopy (TEM), energy-dispersive X-ray spectroscopy (EDX), and Fourier-transform infrared spectroscopy (FTIR) were used to characterize the produced nanocomposite (NC). EDX and TEM analyses revealed the presence of Cu, Fe, and O elements. The NC had a polygonal shape with sides around 12 nm, spherical CuO particles of 7–10 nm, and plate-like Fe2O3. XRD measurements confirmed the crystal and hexagonal structures of CuO and Fe2O3. The XRD patterns of CuO/Fe2O3 showed the characteristic peaks of (−111) and (004) reflections for CuO at 35.69° and 37.73°. The FTIR spectra showed characteristic lines at 525 and 567 cm−1 for the Cu–O bond and Fe–O stretching modes of Fe2O3, respectively. The antifungal activity of CuO/Fe2O3-NCs showed significant growth inhibition of Fusarium oxysporum, Rhizoctonia solani, and Botrytis cinerea by up to 71, 50, and 81%, respectively, at 100 µg/mL. At 50 µg/mL, the antibacterial test revealed inhibition zones of 12.33 mm for Pectobacterium carotovorum, 9.33 mm for Streptomyces scabies, 10.67 mm for Pectobacterium atrosepticum, and 14.67 mm for Ralstonia solanacearum. The results show that CuO/Fe2O3-NCs can efficiently suppress the growth of various fungal and bacterial strains, making them potential antimicrobial agents against phytopathogenic microorganisms.

Molecular origin of viscoelasticity and influence of methylation in mesophase pitch

The viscoelastic and thermomechanical properties of pitches are responsible for their melt-spinning behavior, a critical step for manufacturing high-performance pitch-based carbon fibers. Here, we systematically explore the impact of methyl group modifications on the viscoelastic and thermal properties of mesophase pitches. We employ a range of atomistic modeling approaches, including Density Functional Theory (DFT), Density Functional Tight Binding (DFTB), and Classical Molecular Mechanics (MM), to provide detailed insights into the molecular interactions and structural changes. Our results revealed the molecular mechanisms that promote layered structures leading to the anisotropic nature of the viscoelastic behavior of mesophase pitch. Furthermore, we propose a modified molecular representation of naphthalene-based mesophase pitch based on the analysis of x-ray diffraction measurements. This study provides fundamental insights into the molecular structures of mesophase pitch and the role of methyl groups controlling its viscosity, which offer valuable insights into mesophase-based carbon fiber production.

In-plane hard magnetic BaFe12O19 thin films grown on a-plane Al2O3 112¯0 substrates

Ferrimagnetic barium hexaferrite (BaFe12O19) thin films of varying thicknesses were grown on a-plane Al2O3 112̅0 substrates at elevated temperatures using pulsed laser deposition. X-ray diffraction measurements, Raman spectroscopy, and atomic force microscopy analyses were used to investigate the BaFe12O19 film growth and structure. The results indicate that the formation of an α-Fe2O3 ‘bridge layer’ promotes the growth of a BaFe12O19 phase showing an in-plane uniaxial magnetic anisotropy with an easy-axis of magnetization along the [ 0001 ] hexagonal c-axis direction. The crystallographic relationship between the existing phases is given by BaFe12O19 101̅0 //α-Fe2O3 112̅0 //Al2O3 112̅0. As the thickness increases, the fraction of the BaFe12O19 phase increases further. This is accompanied by a change in grain morphology turning from a columnar to a more elongated shape, where the short axis of the BaFe12O19 grains points along the [ 0001 ] easy axis direction.

Phase analysis of near equiatomic bulk FeRh alloys: X-ray versus neutron diffraction and magnetization measurements

The information obtained by X-ray diffraction (XRD) by impinging the X-ray beam onto the flat surface of bulk Fe–Rh alloys is contrasted with that provided by the thermomagnetic analysis curves measured under a magnetic field of 5 mT and 2 T, and the neutron diffraction (ND) patterns. The experiments were performed on slices cut from bulk Fe50Rh50 and Fe49Rh51 alloys prepared by induction melting followed by 48 h of thermal annealing at 1273 K. Whereas ND patterns and magnetization curves, directly and indirectly point out that the samples are single-phase with a CsCl-type crystal structure undergoing a magnetoelastic transition that changes the magnetic structure from antiferromagnetic to ferromagnetic on heating, multiple phases are identified in the XRD patterns, which modify upon polishing or etching the surface with a mixture of hydrochloric (HCl) and nitric acid (HNO3) at a volume ratio of 90:10 from 30 to 210 min. The limitation of XRD for accurately characterizing the phase constitution within the bulk of Fe–Rh alloys is underlined.

Green Synthesis, Spectroscopic, Electrochemical and Antifungal Characteristics of Ni-doped CeO2 Nanoparticles

This study intended to synthesize Nickel-doped Cerium oxide (Ni-CeO2 NPs) nanoparticles using Pedalium Murex leaf extract. X-ray diffraction (XRD) was used to investigate the structure of the Ni-CeO2 NPs. The XRD measurements showed that the Ni-CeO2 NPs crystallized into the face-centered cubic system. The Ni(1%)-CeO2 and Ni(3%)-CeO2 NP’s crystallite sizes were between 47[Formula: see text]nm and 59[Formula: see text]nm. FTIR and Raman spectral studies were conducted to investigate the sample’s atomic vibrations and chemical bonding. Energy-dispersive X-ray study and field-emission scanning electron microscopy were performed to examine the surface texture and chemical assembly of the Ni-CeO2 NPs. UV–Vis DRS spectrum study was performed to ascertain the reflectance characteristics and bandgap of Ni-CeO2 NPs. The Ni(1%)-CeO2 and Ni(3%)-CeO2 NPs were found to have bandgaps of 2.73[Formula: see text]eV and 2.82[Formula: see text]eV, respectively. Electrochemical impedance spectroscopy and cyclic voltammetry were employed to explore the electrochemical nature of Ni-CeO2 NPs and their capacitive properties at various scanning rates. Using the agar well-diffusion technique, the antifungal activities of Ni-CeO2 NPs were assessed. The experimental findings illustrate the utility of Ni-CeO2 NPs for supercapacitor electrode material and healthcare applications.

Fabrication of Al/n-GaN/p-Si/Al diodes by thermal evaporation and evaluation of effect of gamma irradiation on device properties

This study investigates the impact of γ-irradiation on the material and device properties of Al/n-GaN/p-Si/Al heterojunction diodes. GaN thin films were deposited on glass and p-Si substrates using thermal evaporation, followed by annealing at 450 °C. The diodes were subjected to γ-irradiation doses of 0, 3, and 6 kGy. X-ray diffraction (XRD) measurements revealed significant structural changes, including phase transitions influenced by radiation. Electrical characteristics were assessed through current–voltage (I-V) measurements within the ± 2 V range. Notably, the ideality factor for the annealed diodes improved from 6.60 to 4.62 and 3.85 with increased γ-irradiation. The barrier height was determined to be 0.85 eV, and it did not exhibit a significant change upon γ-irradiation dose. The results provided valuable insights into the response of heterojunction diodes to radiation exposure, aiding in the understanding and potential improvement of the radiation resistance of GaN-based electronic devices.

A Thermally Populated Germylene-Based Donor-Acceptor Diradical.

This work reports synthesis of a germylene based donor-acceptor molecule and its thermal excitation to a triplet state by coordination with a Lewis acid. Products have been characterized by single crystal X-ray diffraction, EPR spectroscopy, and SQUID measurement, in conjunction with DFT calculation. The singlet-triplet energy gap of the donor-acceptor molecule is dramatically reduced from -18.8 to -7.2 kcal/mol by the coordination with B(C6F5)3 (BCF), which enables an intramolecular single electron transfer from one germylene moiety to another upon heating, forming an intramolecular radical ion pair with diradical character. The work provides an approach to the formation of thermally populated open-shell species of heavier main group elements.

Unconventional charge density wave in a kagome lattice antiferromagnet FeGe

FeGe is a kagome material that exhibits both charge density wave (CDW) order and magnetic order. The CDW order is developed deep inside the A-type antiferromagnetic phase in FeGe, providing a unique platform to investigate the interplay between CDW and magnetism. However, the driving mechanism of the CDW phase remains controversial. In this work, we performed high-pressure electrical transport and x-ray diffraction measurements combined with density-functional theory calculations to investigate the evolution of the CDW of FeGe under pressure. In contrast to conventional CDW materials, the CDW transition temperature of FeGe increases with increasing pressure, indicating the unconventional mechanism of CDW in this material. More interestingly, another possible CDW with a 3×3×6 superlattice emerges above 20 GPa, which may be explained by the calculated metastable CDW states under high pressure. These observations exclude the possibility of Van Hove singularities nesting as a CDW driving force. Our results unveil versatile CDW states and broaden the study of intertwined electronic states in the magnetic kagome metal FeGe. Published by the American Physical Society 2024

Physicochemical Characterization and Antimicrobial Properties of Lanthanide Nitrates in Dilute Aqueous Solutions.

This work presents the results of studying dilute aqueous solutions of commercial Ln(NO3)3 · xH2O salts with Ln = Ce-Lu using X-ray diffraction (XRD), IR spectroscopy, X-ray absorption spectroscopy (XAS: EXAFS/XANES), and pH measurements. As a reference point, XRD and XAS measurements for characterized Ln(NO3)3 · xH2O microcrystalline powder samples were performed. The local structure of Ln-nitrate complexes in 20 mM Ln(NO3)3 · xH2O aqueous solution was studied under total external reflection conditions and EXAFS geometry was applied to obtain high-quality EXAFS data for solutions with low concentrations of Ln3+ ions. Results obtained by EXAFS spectroscopy showed significant contraction of the first coordination sphere during the dissolution process for metal ions located in the middle of the lanthanide series. It was established that in Ln(NO3)3 · xH2O solutions with Ln = Ce, Sm, Gd, Yb (c = 134, 100, 50 and 20 mM) there are coordinated and, to a greater extent, non-coordinated nitrate groups with bidentate and predominantly monodentate bonds with Ln ions, the number of which increases upon transition from cerium to ytterbium. For the first time, the antibacterial and antifungal activity of Ln(NO3)3 · xH2O Ln = Ce, Sm, Gd, Tb, Yb solutions with different concentrations and pH was presented. Cross-relationships between the concentration of solutions and antimicrobial activity with the type of Ln = Ce, Sm, Gd, Tb, Yb were established, as well as the absence of biocidal properties of solutions with a concentration of 20 mM, except for Ln = Yb. The important role of experimental conditions in obtaining and interpreting the results was noted.

Effect of Carbon Content on the Phase Composition, Microstructure and Mechanical Properties of the TiC Layer Formed in Hot-Pressed Titanium-Steel Composites

During the hot pressing of pure titanium and different carbon steels in a temperature range of ϑ = 950–1050 °C, a compound layer up to dL≈10 μm thick is formed at the titanium–steel interface. With a higher carbon content of the used steel, the layer thickness increases. The carbon concentration within the layer is in the range of stoichiometry for TiC. Apart from TiC, no other phases can be detected by X-ray diffraction (XRD) measurements inside the formed layer. The calculation of the activation energy for the TiC layer formation is Q = 126.5–136.7 kJ mol−1 and is independent of the carbon content of the steel. The resulting microstructure has a grain size gradient, wherein the mechanical properties, such as hardness and Young‘s modulus, are almost constant. Statistical analysis using Response Surface Methodology (RSM) indicates that the carbon content of the steel has the most significant influence on layer thickness, followed by annealing temperature and annealing time. By selecting the appropriate carbon steel and the subsequent removal of the steel, it is possible to produce targeted TiC layers on titanium substrates, which holds enormous potential for this material in wear-intensive applications.

Copper (II) halide compounds with cationic N-donor ligands: Design, synthesis, structure and magnetism

Copper (II) complexes of the cationic ligands 1-(4′-pyridyl)-pyridinium (L1) and 1-(4′-pyridyl)-pyridin-4-ol (L2) have been prepared and characterized by single crystal X-ray diffraction and variable temperature magnetic susceptibility measurements: [Cu(L1)2X2]X2 [where X = Cl (1), Br (2)], and [Cu(L2)2X2]X2 [where X = Cl (3), Br (4)]. The complexes are fundamentally square planar with L2X2 coordination planes and long, semi-coordinate bonds to the additional halide ions. All compounds crystallize in monoclinic systems with 1 and 2 in the P21/n space group and 3 and 4 in the P21/c space group. The crystal structures are stabilized by both non-classical (in the case of 1 and 2) and classical (3 and 4) hydrogen bonds. EPR data for 1–4 support a rhombohedral structure, in good agreement with the local geometry as seen in the crystal structures. Magnetic susceptibility measurements show the presence of very weak antiferromagnetic interactions. In addition, the syntheses and magnetic properties of two neutral complexes, [Cu(L3)2X2]·2H2O [L3 = 1-(4′-pyridino)-4-pyridone; X = Cl (5), Br (6)] are reported. Magnetic susceptibility data indicate the presence of moderate antiferromagnetic exchange interactions [J ∼ 28 K (5), 60 K (6)] which were well modeled by the S = 1/2 Heisenberg uniform chain model.

Oxidation and compositional modulation in single phase C14 Zr0.6Ti0.4Fe1Cr1 alloy

This study investigates the effects of heat treatment on the crystal structure and hydrogen absorption behavior of the AB2 type metal hydride Zr0.6Ti0.4Fe1Cr1. The objective is to understand how 3- and 6-day heat treatments at 1000°C influence the alloy's microstructure and hydrogenation properties. Using electron microscopy, EBSD analysis, X-ray diffraction, and hydrogenation measurements, we found that the as-cast alloy exhibits rapid hydrogen absorption with significant compositional variations due to segregation during casting, confirmed by a single C14 Laves phase in XRD. Heat treatment slowed hydrogen absorption and reduced hydrogen capacity, with XRD indicating the structure remained primarily C14 Laves phase. However, SEM/EDS analysis showed substantial microstructural changes, including the emergence of new phases and segregation of Zr-rich phases, likely non-hydride forming, influenced by elevated oxygen content. These new phases probably contribute to the reduced hydrogen uptake capacity.

Fluorinated Amide-Based Electrolytes Induce a Sustained Low-Charging Voltage Plateau under Conditions Verifying the Feasibility of Achieving 500 Wh kg-1 Class Li-O2 Batteries.

Although lithium-oxygen batteries (LOBs) hold the promise of high gravimetric energy density, this potential is hindered by high charging voltages. To ensure that the charging voltage remains low, it is crucial to generate discharge products that can be easily decomposed during the successive charging process. In this study, we discovered that the use of amide-based electrolyte solvents containing a fluorinated moiety can notably establish a sustained voltage plateau at low-charging voltages at around 3.5 V. This occurs under conditions that can verify the feasibility of achieving a benchmark energy density value of 500 Wh kg-1. Notably, the achievement of the low-voltage plateau was accomplished solely by relying on the intrinsic properties of the electrolyte solvent. Indeed, synchrotron X-ray diffraction measurements have shown that the use of fluorine-containing amide-based electrolyte solvents results in the formation of highly decomposable discharge products, such as amorphous and Li-deficient lithium peroxides.

From Chitin Nanowhisker Colloidal Dispersions to Anisotropic Microfibers: Structural Evolution in Its Transformation Process as Revealed by Synchrotron Wide-Angle X-ray Diffraction Measurements.

Nanowhiskers in a colloidal dispersion are known to form chiral nematic liquid crystals (CNLC), as seen in a cellulose nanowhisker or so-called cellulose nanocrystal and chitin nanowhisker. In our related work, we clarified that once the thus-created chitin nanowhiskers with surface modified by chitosan (CTWK-CS) in CNLC phase were wet-spun, we could directly obtain anisotropic microfibers containing the highly ordered CTWK-CS. This drastic structural transformation from CNLC to anisotropic microfibers might relate to several important stages, i.e., stage (i) is the alignment of CTWK-CS initiated by a specific concentration and flow to create aggregation in the CNLC state, stage (ii) is the coagulation of CTWK-CS in CNLC to transform to microfibers, and stage (iii) is the drying of the thus-extruded microfibers to allow CTWK-CS alignment. The present work sets up the experimental systems simulating stages (i) and (iii) to reveal the orientational behavior of CTWK-CS and the structural evolution, respectively, by synchrotron 2D WAXD measurement. In stage (i), the high degree of the parallel alignments of CTWK-CS with the chain axis oriented along the flow direction of the colloidal dispersions confirms that the flow and concentration synergistically controlled CTWK-CS alignment. In contrast, for stage (iii), the poor c-axial orientation of CTWK-CS in as-spun wet microfibers gradually changed to the high degree of c-axial orientation along the fiber direction during drying process, indicating a reorientation of CTWK-CS along with dehydration. The present study declares an in situ observation of the direct wet spinning of nanowhiskers about their remarkable alignments in the sheared colloidal dispersions (stage (i)) and their random-to-high reorientation during the drying process of the as-spun wet microfiber (stage (iii)).

Effect of welding residual stresses on the fatigue life assessment of welded connections

Welding residual stresses impose significant influences on the fatigue behavior and structural integrity of welded connections in various engineering applications. Understanding the effects of these residual stresses on fatigue life is crucial for ensuring the reliability and safety of welded structures. This paper proposes a damage-incorporated thermal–mechanical simulation method to examine the effect of welding residual stresses on the fatigue life prediction of welded plates and circular hollow section (CHS) X-joints. Compared to the experimental X-ray diffraction measurements and the fatigue tests, the predicted residual stresses and fatigue life demonstrate good agreement with experimental results for both high-cycle and low-cycle fatigue. The location of fatigue cracks resembles closely the estimation from a uniform fatigue damage indicator. The fatigue life prediction without incorporating the welding residual stresses does not affect significantly the life estimation for low-cycle fatigue but can cause substantial over-predictions for high-cycle fatigue.

Analysis of Lattice Damage in 4H-SiC Epiwafers Implanted with High Energy Al Ions at Elevated Temperatures

4H-SiC wafers with 12 µm epilayers were blanket implanted to a depth of 12 µm with 5 x 1016 cm-3 Al ions via Tandem Van de Graaff accelerator located at Brookhaven National Laboratory with energy range of 13.8 to 65.7 MeV at room temperature, 300 °C and 600 °C. High resolution X-ray diffraction measurements reveal the implanted layers are characterized by tensile strains. However, the dynamic annealing process reduces the level of tensile strains as the temperature of implantation is increased. Analysis indicates that the implant temperature of 600 °C is not sufficient to minimize lattice damage due to implantation and a higher implantation temperature will be required. This preliminary experiment will guide the optimization of implantation conditions for fabricating superjunction devices.

Effects of heat treatment on the microstructure and corrosion behavior of manganese aluminum bronzes

Abstract Due to a much lower nickel content, manganese aluminum bronzes (MAB) are a cost-effective alternative to nickel aluminum bronzes (NAB). When the material is processed, different microstructures are observable in the material which have an impact on the corrosion resistance of MAB alloys. MAB samples were annealed at 900 °C and quenched in water. After that, annealing treatments at 600, 500, 400 and 300 °C for up to 24 h were performed and the samples were again quenched in water. Metallographic sections were prepared from all samples and potentiostatic corrosion tests at different potentials were performed in synthetic seawater. It was found that the sample annealed at 900 °C and quenched in water as well as those samples which underwent a second annealing treatment at low temperatures for shorter times exhibited a greater corrosion tendency than those undergoing a second annealing treatment at higher temperatures. X-ray diffraction measurements revealed that phase transformations and changes in grain size occurred during the annealing treatments. The increase in corrosion resistance as a result of annealing at higher temperatures is probably due to the strong intergrowth of the phases that are formed.

Characterization and application of electrochemical deposition Cdse thin films

The electrochemical deposition method created a CdSe thin film on FTO glass substrates. The film was examined using field scanning electron microscopy, energy dispersive spectroscopy, X-ray diffraction, Raman spectroscopy, and optical and electrochemical measurements. The results show that the CdSe nanoparticles were evenly distributed on the substrate, with a Cd/Se ratio of 63.30% Se and 36.70% Cd. The XRD revealed a polycrystalline, hexagonal structure. The film is n-type semiconductor concentration with a carrier concentration of 1.194×1020 cm-3 . The CdSe showed 552.5 mF/cm2 of specific capacity with energy and a power density of 2.5 mW/cm2 and 9000 mW/cm2 , respectively